Knauer BlueShadow Detector 10D User manual

Detector 10D
User Manual
V7670
HPLC
BlueShadow

3TableofContents
KNAUER Detector 10D User Manual V7670A, Version 2.3
Table of Contents
Note For your own safety, be sure to read the manual and always
observe the warnings and safety information on the device and
in the manual!
Intended Use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Device Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
Features . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
Eluents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Scope of Delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
Safety for Users . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
Definition of Personal and Material Damage . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Symbols and Signs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Unpacking and Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Contacting the Technical Support . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Location Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Space Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Unpacking . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Connectors on the Rear Side . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Spring Strip for Remote Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Plug Connector Assignments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
Connecting Cables to the Pin Header . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
Analog Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Ground . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Initial Startup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Inserting the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Setting the Optical Path Length of a Preparative Flow Cell . . . . . . . . . . . . . . . 21
Connecting the Capillaries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Startup of the Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Operation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Basic Operation of the Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Control of the Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
Menu Structure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Control . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Activating/Deactivating the Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Adjusting the Chromatogram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Smoothing output signal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Adjusting V/AU ratio . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Checking on the Deuterium Lamp . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Displaying Operating Hours . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Using the Analog Port . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Setting the Zero Point . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

4TableofContents
KNAUER Detector 10D User Manual V7670A, Version 2.3
Entering a Scaling Value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Control with Chromatography Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
Local Area Network (LAN) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Serial interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
Functionality Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
Maintenance and Care. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Maintenance Contract . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
Cleaning and Caring for the Device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
What Maintenance Tasks can Users Perform on the Device? . . . . . . . . . . . . . . 32
Cleaning the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Rinsing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Cleaning the Lens of an Analytical Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . 34
Cleaning the Light Guide of a Preparative Flow Cell . . . . . . . . . . . . . . . . . . 35
Replacing the Flow Cell . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Replacing the Fiber Optic . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
Removing the Fiber Optics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
Technical Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
Legal Information . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Warranty Conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Transport Damage . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Disposal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Decontamination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
Index . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
Declaration of Conformity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44

5IntendedUse
KNAUER 10D User Manual V7670, Version 2.3
Intended Use
Note Only use the device for applications that fall within the range of
the intended use. Otherwise, the protective and safety equip-
ment of the device could fail.
Device Overview
The detector is a measuring device that is used for measuring UV
spectra quickly and precisely.
Operating range The detector can be used in analytical and preparative HPLC sys-
tem. It is used in laboratories to analyze substance mixtures. In
an HPLC system, the detector serves to detect substances in liq-
uids and show their concentration.
In laboratories the device can be used in the following areas:
Separation of chiral substances
1Display
2Function button 1
3Function button 2
4Autozero button
5Flow cell
Fig. 1 Detector Front view
6RS-232 port
7LAN port
8Spring strip
9Integrator output
bl Power connection
bm Ground connection
bn Fan opening on rear
panel
Fig. 2 Detector Rear view
4
123
5
6
7
8
9
bl
bm
bn

6IntendedUse
KNAUER 10D User Manual V7670, Version 2.3
Separation of proteines
Separation of fine chemicals
Separation of active pharmaceutical ingredients (API)
The detector is, e. g., used at universities, research institutions,
and routine laboratories.
Features
This detector is one of the smallest HPLC detectors on the
market.
With the deuterium lamp spectra from
190 nm – 500 nm can be measured.
Flexible use in the entire range of HPLC: Analytical flow cells
with ≈10-μl/min flow rates and preparative flow cells with10-
l/min flow rates.
Automatical recognition and storing of device-specific infor-
mation, which are important for Good Laboratory Practice,
operation qualifications, or repairing the device Operation
Qualification) or for repairing the device
Automatic and current diagnosis of the device.
External control with chromatography software or membrane
keyboard
Easy integration of the detector into complex chromatogra-
phy systems
Options Various types of flow cells are available to the user. Pay attention
to the compatability of the flow cells.
A test cell is preassembled to the detector. Before the detector
can be used, the test cell has to be replaced by a flow cell. The
fiber optics detector is delivered without a test cell.

7IntendedUse
KNAUER 10D User Manual V7670, Version 2.3
Eluents
Even small quantities of other substances, such as additives,
modifiers, or salts can influence the durability of the materials.
The solvent list contains the solvents KNAUER recommends for
use. If there is any doubt, contact the Technical Support of the
manufacturer.
Suitable solvents
Acetic acid (10–50 %) at 25 °C/77.0 °F
Acetone at 4 °C–25 °C (39.2 °F–77.0 °F)1
Acetonitrile
Ammonia
Benzene
Carbon dioxide (liquid 99.999 % CO2)
Chloroform
Dilute ammonia solution
Dilute sodium hydroxide (1 M)
Ethyl acetate
Ethanol
Hexane/heptane
Isopropanol
Methanol
Phosphate buffer solutions (0.5 M)
Phosphoric acid
Sodium hydroxide
Toluol
Water
1. valid for the specified temperature range
Less suitable solvents
Dimethyl sulfoxide (DMSO)
Methylene chloride
Slightly volatile solvents
Tetrahydrofuran (THF)

8IntendedUse
KNAUER 10D User Manual V7670, Version 2.3
Not suitable solvents
Bases
Halogenated hydrocarbons, e.g. Freon®
Mineral and organic acids (except in buffer solutions)
Perfluorinated solvents, e.g. Fluorinert®FC-75, FC-40
Perfluorinated polyether, e.g. Fomblin®
Solvents containing particles

9ScopeofDelivery
KNAUER 10D User Manual V7670, Version 2.3
Scope of Delivery
Note Only use original parts and accessories made by KNAUER or a
company authorized by KNAUER.
Delivery Detector with flow cell1
Power Cable
Power unit
Accessories kit UV-Detector 10D
User manual (DE/EN)
Installation Qualification Document (DE/EN)
transportation securing device (standard detector)
1. A test cell is not included with the fiber optics detector delivery.

10 Safety for Users
KNAUER 10D User Manual V7670, Version 2.3
Safety for Users
Professional group The user manual is addressed to persons that are qualified as
chemical laboratory technicians or have completed comparable
vocational training.
The following knowledge is required:
Basic knowledge of liquid chromatography
Knowledge regarding substances that are suitable only to a
limited extent for use in column liquid chromatography
Knowledge regarding the health risks of chemicals
Participation during an installation of a device or a training by
the company KNAUER or an authorized company.
If you do not belong to this or a comparable professional group,
you may not perform the work described in this user manual
under any circumstances. In this case, please contact your supe-
rior.
Personal Safety Equip-
ment for Professional
Group
When working with the device, take measures according to lab
regulations and wear protective clothing:
safety glasses with side protection
protective gloves
overall
What must be taken into
account?
All safety instructions in the user manual
The environmental, installation and connection specifications
in the user manual
National and international regulations pertaining to labora-
tory work
Original spare parts, tools, and eluents made or recom-
mended by KNAUER
Good Laboratory Practice (GLP)
For development of methods and validation of devices: Pro-
tocol for the Adoption of Analytical Methods in the Clinical
Chemistry Laboratory, American Journal of Medical Technol-
ogy, 44, 1, pages 30-37 (1978)
Accident prevention regulations published by the accident
insurance companies for laboratory work
More safety-relevant information is listed in alphabetical order in
the following table:
Topic Explanations
Decontamination Contamination of devices with toxic, infectious or radioactive
substances poses a hazard for all persons during operation,
repair, sale, and disposal of a device. All contaminated devices
must be properly decontaminated. All materials or fluids used
for decontamination must be collected separately and dis-
posed of properly.

11 Safety for Users
KNAUER 10D User Manual V7670, Version 2.3
Where is use of the
device prohibited?
Never use the system in potentially explosive atmospheres with-
out appropriate protective equipment. For further information,
contact the Technical Support of KNAUER (see See “Contacting
the Technical Support” on page 13.).
Take the device out of
operation
At any time, take the device completely out of operation by
either switching off the power switch or by pulling the power
plug.
Opening the module The device may only be opened by the Technical Support of the
manufacturer or any authorized person (see See “Contacting the
Technical Support” on page 13.).
Flammability Organic eluents are highly flammable. Since capillaries can
detach from their screw fittings and allow eluent to escape, it
is prohibited to have any open flames near the analytical sys-
tem.
Leaks Regularly check if any system components are leaking.
Solvent tray Risk of electrical shock or short circuit if liquids get into the
device's interior. For this reason, place all bottles in a solvent
tray.
Eluent lines Install capillaries and hoses in such a way that liquids cannot
get into the interior in case of a leak.
Power strip If several devices are connected to one power strip, always
consider the maximum power consumption of each device.
Power cable Defective power cables are not to be used to connect the
device and the mains power.
Self-ignition point Only use eluents that have a self-ignition point higher than
150 °C under normal ambient conditions.
Power supply Only connect devices to voltage sources, whose voltage
equals the device's voltage.
Toxicity Organic solvents are toxic above a certain concentration.
Ensure that work areas are always well-ventilated! Wear pro-
tective gloves and safety glasses when working on the device!
UV light Concentrated UV light can disperse from a detector without
flow cell or from the optical fiber, which leads to irritation of
the retina. When the flow cell or the fiber optic are replaced,
switch the device off and pull the power plug.
Topic Explanations

12 Safety for Users
KNAUER 10D User Manual V7670, Version 2.3
Definition of Personal and Material
Damage
Possible dangers related to the device are distinguished in per-
sonal and material damages in this user manual.
Type of damage Category Explanations
Personal damages DANGER! Lethal or very serious injuries can occur.
WARNING! Serious injuries can occur.
Personal and material dam-
age
CAUTION! Moderate injuries can occur.

13 Symbols and Signs
KNAUER 10D User Manual V7670, Version 2.3
Symbols and Signs
The following symbols and signs can be found on the device, in
the chromatography software or in the user manual:
Symbol Meaning
High-voltage hazard
Electric shock hazard
Electrostatic discharge hazard, damages
to system, device, or components can
occur.
General warning sign, moderate injuries
can occur and also damages to system,
device, or components.
UV-light hazard, eye injuries can occur.
A device or system marked with CE fulfills
the product specific requirements of Euro-
pean directives. This is confirmed in a
Declaration of Conformity.

14 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Unpacking and Setup
Contacting the Technical Support
You have various options to contact the Technical Support:
Phone [phone]
Fax [phone]
E-mail [email protected]
You can make your requests in English and German.
Location Requirements
Power supply The device is only suitable for 24 V direct current.
Only the supplied power unit is to be used to connect the device
to the mains supply. Replace defective power unit only with
original accessories from KNAUER.
Only use power units with a permission for use from your coun-
try. In case of queries contact the Technical Support.
Power Plug
Note Make sure that the power plug on the rear of the device is
always accessible, so that the device can be disconnected from
the power supply.
Requirements The location for the device must meet the following require-
ments:
CAUTION!
Defect of the device due to overheating possible!
Protect the device against exposure to direct sun-
light.
Keep clear at least 15 cm at the rear and 5–10 cm
at each side for air circulation.
level surface for device or system
Protect from heavy ventilation
Weight 1.5 kg
Dimensions 121 x 129 x 187 mm
(width x height x depth)
Power Supply 24 V DC
Air humidity below 90 %, non condensing
Temperature
range
4 – 40 °C
39.2 – 104 °F

15 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Space Requirements
Side clearance to other devices:
At least 5 cm, if there is another device on one side.
At least 10 cm, if there are devices set up on both sides.
At least 15 cm on the rear panel for the fan.
Unpacking
Store all packing material. Retain included packing list carefully
for repeat orders.
Tool Utility knife
CAUTION!
Schäden an der Durchflusszelle durch falsches
Heben möglich!
Den Detektor seitlich am Gehäuse hochheben.
Procedure 1. Check for damage caused during transportation. In case you
notice any damage, contact the Technical Support and the
forwarder company.
2. Setup the delivery in such a way that the label is in the cor-
rect position. Using the utility knife, cut the adhesive tape.
Open the packaging.
3. Remove the foam insert. Take out the accessories kit and the
manual.
4. Open the accessories kit and take out all accessories. Check
the scope of delivery. In case any parts are missing, contact
the Technical Support.
5. Clasp the device at its side panels and lift it out of the packag-
ing.
6. Remove the foam inserts from the device.
7. Check for damage caused during transportation. In case you
notice any damage, contact the Technical Support.
8. Set up the device in its location.
9. Remove protective foil and transportation securing device
(standard detector).

16 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Connectors on the Rear Side
All connectors are located on the rear side of the detector.
External devices like computers, fraction collectors, etc. can be
connected in 3 different ways to the detector:
Connected via the spring strip (remote connector)
Connected via LAN within a network
Connected via RS-232
Spring Strip for Remote Control
CAUTION!
Zerstörung der Elektronik durch elektrostatische
Entladung!
Geerdetes Armband tragen.
The spring strip is used for remote control. The single ports
transport start, control and error signals.
Plug Connector Assignments
Legend
1RS-232 port
2LAN port
3Spring strip
4Analog port
5Power connection
6Ground
7Fan
Fig. 3 Detector Rear view
1
2
3
4
5
6
7
Connector Function
GROUND Reference point of the voltage at the
signal inputs.
AUTOZERO A signal (short-circuit to GROUND)
sets the measuring signal to zero.

17 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Connecting Cables to the Pin Header
To control one device through another, you use the pin header.
The single ports are used to exchange control signals.
To use remote control, you have to connect cables to the pin
header. Therefore, connect the cables firstly to the spring strip
and push the spring contacts of the spring strip secondly onto
the pins of the pin header.
Prerequisites The device has been turned off.
The power plug has been pulled.
Tools Depressor tool
CAUTION!
Short-circuit hazard.
Turn off the device before connecting it to the
pin header. Pull the power plug.
CAUTION! Electrostatic discharge can destroy the
electronics!
Wear protective bracelet against electrostatic dis-
charge and ground.
ERROR IN/OUT IN: After receiving a signal (short-cir-
cuit to GROUND) from an external
device, an error message appears and
the device stops.
OUT: An error signal is active for as
long as an error is displayed e.g. the
lamp does not start.
GROUND Reference point for external analog
control of the detector.
ANALOG IN Allows external analog control of the
detector when the option ANALOG
has been selected in the SETUP menu.
The control voltage must be applied
against GROUND.
Start IN After receiving a signal (short-circuit to
GROUND) from an external device,
the device starts. If controlled via soft-
ware, an electronic trigger is sent via
LAN.
Connector Function

18 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Next steps Finish the installation and perform the initial startup.
Analog Port
Using the analog port (ANALOG-IN), you can control the wave-
length by changing the applied voltage. Before connecting the
analog port, you have to choose analog in the setup menu. The
control voltage must be applied against GROUND. (see See
“Using the Analog Port” on page 27.)
Example To use the analog port for controlling the detector, you have to
set a zero point and enter a scaling value.
Zero point at 0 V = 000 nm
Scaling: 100 nm per Volt
If 5-V voltage is applied, the wavelength is 500 nm.
Ground
Note The detector is not grounded if it is connected with a 24-V
power supply to a 220-V outlet.
Voltages, which may influence the measuring result, can be dis-
charged if the device is detected to a grounded KNAUER device,
e. g., a thermostat.
Tool Depressor tool
Procedure Process Figure
1. Place the spring strip 3
on a suitable surface.
2. Push the depressor tool 1
into the opening on the
spring strip.
3. Continue pushing the
depressor tool down and
lead the cable 2into the
front end of the spring
strip.
4. Remove the depressor
tool.
5. Check whether the cables
are tightly attached.
6. Plug the spring strip onto
the pin header.
Fig. 4 Spring strip
1
2
3

19 Unpacking and Setup
KNAUER 10D User Manual V7670, Version 2.3
Process Figure
Procedure 1. Remove 5 mm of insula-
tion from the ends of the
cable 2.
2. Using the depressor tool,
open the port Ground 1
on the spring strip.
3. Insert the first cable end.
4. Connect the second cable
end to the port Ground on
the remote connector of a
grounded 220-V KNAUER
device 3.
Result The physical connection is established.
1
2
3

20 Initial Startup
KNAUER 10D User Manual V7670, Version 2.3
Initial Startup
Note Before the detector is ready to use, a flow cell must be installed.
Before installing the flow cell, the optical path length can be
changed. The optimal path length depends on type and quan-
tity of the sample.
Inserting the Flow Cell
The test cell has no connectors for capillaries and must therefore
be replaced by a flow cell before first usage.
Note The test cell is used during operation qualifications and must be
stored.
Prerequisite Detector has been switched off.
Power plug is pulled out.
Process Figure
Procedure 1. Unscrew the 2 knurled-
head screws 1.
2. Pull out the slide 2.
3. Remove the test cell.
Fig. 5 Removing the slide
4. Insert the flow cell 4
into the slide 3.
5. Push the slide into the
detector.
6. Insert the knurled-head
screws and screw tight.
Fig. 6 Assembling the flow cell
Result Flow cell is assembled. The next step is connecting the capil-
laries.
1
2
3
4

21 Initial Startup
KNAUER 10D User Manual V7670, Version 2.3
Setting the Optical Path Length of a
Preparative Flow Cell
WARNING!
Irritation of retina through UV light! Concen-
trated UV light can leak out from the flow cell or
the fiber optic connectors.
Switch off the device and pull the power plug.
Depending on type, the path length is factory set to 2 mm,
3 mm, or 10 mm. You can remove the spacers on one or both
sides and hence change the path length to 1.25 mm or 0.5 mm.
Prerequisite Flow cell has been disassembled.
Tool Allen wrench size 3
Procedure 1. Using the allen screwdriver, unscrew and remove the
threaded ring 1.
2. Remove the cover 2and spacer 3. Put the spacer aside.
3. Insert the cover.
4. Using the wrench, tighten the threaded ring.
Extending the Optical
Path Length
To enlarge the optical path length, put in one or both spacers.
Legend
1Threaded ring
2Cover
3Spacer
4Seal holder (com-
pression bushing)
5Light guide with
PTFE seal
Fig. 7 Preparative flow cell
1
2
3
4
5